関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(2-Bromo-chlorobenzoyl)-2,3-dihydro-4-pyridinone | HCID 22008820 | — |
| 触媒 | Palladium(2+) acetate--triphenylphosphane (1/2/2) | HCID 84538 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (+/-)-7-Chloro-1,3,4,10b-tetrahydropyrido[2,1-a]isoindole-2,6-dione | HCID 22008819 | 31.1% |
反応手順
A mixture of 1-(2-bromo-chlorobenzoyl)-2,3-dihydro-4-pyridinone (Preparation 3) (300 mg, 0.954 mmol), triethylamine (0.39 mmol, 0.54 ml), formic acid (0.05 ml, 1.3 mmol) and di(triphenylphosphine) diacetoxypalladium (47 mg, 0.063 mmol) in DMF (3 ml) was heated to 80° C. for 2 h. The cooled solution was filtered through celite, diluted with water, extracted twice with ethyl acetate, the extracts dried over sodium sulphate and evaporated. The residue was purified by flash column chromatography on silica eluting with 50% ethyl acetate in hexane to yield the title compound as a colourless oil (70 mg). MS (+CI) m/z 235/237 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06211189B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-d095710205ce4149af120fea9605be03 |
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| 出典メモ | uspto-grants-2001_04 |
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